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GB 23200.13-2016Food safety national standard -- Determination of residues of 448 pesticides and related chemicals in tea by liquid chromatography-mass spectrometry (English PDF)

茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法

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Issued by

National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

Level / Type

National · Mandatory

Issue date

December 18, 2016

Implementation date

June 18, 2017

Scope

GB 23200.13-2016 is the English-translated version of 茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法.

GB 23200.13-2016 — This standard stipulates that 448 kinds of pesticides and related chemicals (see Appendix A) of the green tea, black tea, Pu'er tea, oolong tea, Determination of Chromatography - Mass Spectrometry.

This standard applies to green tea, black tea, Pu'er tea, oolong tea 448 kinds of pesticides and related chemicals residue qualitative identification, but also for Quantitative determination of 418 pesticide and related chemical residues, other tea can refer to the implementation.

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Document preview — GB 23200.13-2016

National Standard of the People's Republic of China

Classification: G 25
Replacing: GB/T 23205-2008

Issued by: National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration

Preface
1 Scope
2 Normative reference document
Principle
4 Reagents and materials
5 Instruments and equipment
6 Preparation of sample
7 Analysis Step
Calculation and presentation of results
9 Precision
10% limit and recovery rate
Appendix A (informative) 448 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixing
Standard solution concentration Table
Appendix B (informative) 448 Pesticides and Related Chemicals Monitoring Ion Impact Energy, Source Fragmentation Voltage and Retention Time
Appendix C (informative) 448 Pesticides and Related Chemicals Multiple Reaction Monitoring (MRM) Chromatogram
Appendix D (informative) Relative standard deviation in laboratory
Appendix E (informative) Relative standard deviation between laboratories
Appendix F (informative) Experimental data on the concentration and recovery of samples

Foreword

This standard replaces GB/T 23205-2008 "Determination of 448 pesticides and related chemical residues in tea by liquid chromatography - tandem mass Spectrum method ".

This standard compared with GB/T 23205-2008, the main changes are as follows.

- Standard text format is modified to national standard text format for food safety;

- increase the "other tea can refer to the implementation" in the standard range.

This standard replaced the previous version of the standard release.

-GB/T 23205-2008.

National standards for food safety Determination of 448 Pesticides and Related Chemical Residues in Tea Liquid chromatography - mass spectrometry

1 Scope

This standard stipulates that 448 kinds of pesticides and related chemicals (see Appendix A) of the green tea, black tea, Pu'er tea, oolong tea, Determination of Chromatography - Mass Spectrometry.

2 Normative reference documents

The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this article Pieces. For undated references, the latest edition (including all modifications) applies to this document.

GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs GB/T 6682 Analytical laboratory water specifications and test methods

3 Principle

The sample was extracted with acetonitrile and purified by solid phase extraction column. The pesticide and related chemicals were eluted with acetonitrile-toluene solution (3 1) Phase chromatography - tandem mass spectrometry, external standard method.

4 Reagents and materials

Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682.

4.1 Reagents

4.1.1 Acetonitrile (CH3CN, 75-05-8). Chromatographic Purification.

4.1.2 Toluene (C7H8, 108-88-3). Excellent grade pure.

4.1.3 Acetone (CH3COCH3, 67-64-1). Chromatographic pure.

4.1.4 Isooctane (C8H18,540-84-1). Chromatographic pure.

4.1.5 Methanol (CH3OH, 67-56-1/170082-17-4). Chromatographic Purification.

4.1.6 acetic acid (CH3COOH, 64-19-7). excellent grade pure.

4.1.7 Chloride (NaCl, 7647-14-5). Analytical purity.

4.1.8 anhydrous sodium sulfate (Na2SO4,7757-82-6). analytical grade. Before burning at 650 °C for 4 h, stored in a dryer, cooling and standby.

4.2 Solution preparation

4.2.1 0.1% formic acid solution. take 1000 mL of water, add 1 mL of formic acid, shake back standby.

4.2.2 5mmol/L ammonium acetate solution. Weigh 0.385g ammonium acetate, diluted with water to 1000mL.

4.2.3 acetonitrile - toluene solution (3 1). take 300 mL of acetonitrile, add 100 mL of toluene, shake back.

4.2.4 acetonitrile aqueous solution (3 2). take 300 mL of acetonitrile, add.200 mL of water, shake back.

4.3 Standards

Pesticide and Related Chemical Reference Material. Purity >=95%, see Appendix A.

4.4 Standard solution preparation

4.4.1 Standard stock solution

Respectively, weighing 5mg ~ 10mg (accurate to 0.1mg) pesticides and related chemicals in the standard 10mL volumetric flask, according to the standard the solubility of the quasi-selected methanol, toluene, acetone, acetonitrile or isooctane dissolved and constant volume to the scale (solvent options see Appendix A), the standard solution Liquid stored at 4 °C, the shelf life of one year.

4.4.2 Mixing standard solutions (mixed standard solutions A, B, C, D, E, F and G)

According to the retention time of pesticides and related chemicals, 448 kinds of pesticides and related chemicals are divided into A, B, C, D, E, F and G and the concentration of each pesticide and associated chemical in the instrument to determine the concentration in the mixed standard solution. This standard for the group of 448 pesticides and related chemicals and their mixed standard solution concentrations, see Appendix A.

Depending on the grouping of each pesticide and associated chemical, the concentration of the standard solution and the concentration of the standard stock solution, the amount of individual Pesticide and related chemicals Standard stock solution in 100mL volumetric flask, with a fixed volume of methanol to the scale. Mixed standard solution stored at 4 ° C, the shelf life is one month.

4.4.3 Substrate mixed standard working solution

Pesticide and related chemicals Substrate mixed standard working solution is prepared by mixing the sample with different concentrations of the substrate mixed with standard working solution Liquid A, B, C, D, E, F and G are used for standard working curves. Matrix mixed standard working solution should be used with the current distribution.

4.5 Materials

4.5.1 Microporous membrane (nylon). 13 mm × 0.2 µm.

4.5.2 Cleanert TPT

1) solid phase extraction column. 10 mL, 2.0 g, or equivalent.

5 Instruments and equipment

5.1 Liquid Chromatography - Tandem Mass Spectrometer. Equipped with electrospray ion source.

5.2 Analysis of balance. 0.1 mg and 0.01 g.

5.3 chicken heart bottle..200 mL.

5.4 Pipettes. 1 mL.

5.5 Vials. 2 mL, with Teflon Capping.

5.6 with a plug centrifuge tube. 50 mL.

5.7 nitrogen dryers.

5.8 Low speed centrifuge. 4200 r/min.

5.9 Rotary Evaporator.

5.10 high-speed organization of crusher.

6 Sample preparation

The tea samples were sintered in a pulverizer and the samples were passed through a standard screen of 425 µm. Mix, prepare the prepared samples are divided into two, Into a clean sample container, sealed and marked. The samples were cryopreserved at -18 ° C.

7 Analysis steps

7.1 Extraction

Weigh 10g sample (accurate to 0.01g) in 50mL equipped with a centrifuge tube, add 30mL acetonitrile solution, in high-speed tissue crusher on the 15000r/min homogenate extraction 1min, 4200r/min centrifugal 5 min, supernatant into the heart of the bottle. Residue plus 30mL acetonitrile, uniform Pulp 1 min, 4200 r/min centrifugal 5 min, supernatant into the heart of the bottle, the residue plus 20mL acetonitrile, repeat the extraction time, supernatant Into the heart of the bottle, 45 °C water bath, spin concentrated to near dry, nitrogen blowing to dry, add 5 mL of acetonitrile dissolved residue, take 1mL to be net the

7.2 Purification

Add about 2 cm of anhydrous sodium sulfate to the Cleanet-TPT column and place the column on the holder of the flask. Before loading Wash the column with 5 mL of acetonitrile-toluene solution and quickly transfer the sample extract to the purification column when the liquid level reaches the top of the sodium sulfate.

Replacement of new chicken heart bottle. Add a 50 mL reservoir to the Cleanert TPT column and elute pesticide and related chemistry with 25 mL acetonitrile-toluene solution the product was combined in a heart flask and concentrated in a water bath at 45 ° C to about 0.5 mL, dried at 35 ° C under nitrogen, 1 mL of acetonitrile-water solution the residue was filtered through a 0.2 µm microfiltration membrane and analyzed by liquid chromatography-tandem mass spectrometry.

The Cleanert TPT column is the trade name of Agela's products, and this information is intended for the convenience of users of this standard and is not intended to endorse the product. If other equivalent products have the same effect, you can use these equivalent products.

7.3 Determination

7.3.1 Liquid Chromatography - Tandem Mass Spectrometry Reference Conditions

7.3.1.1 Determination of LC-MS-MS for pesticides and related chemicals in Groups A, B, C, D, E and F A) Column. ZORBAX SB-C18, 3.5 µm, 100 mm × 2.1 mm (inner diameter) or equivalent;

B) mobile phase and gradient elution conditions in Table 1;

Table 1 Mobile phase and gradient elution conditions

Total flow/min Flow rate/(µL/min) Mobile phase A (0.1% formic acid) /% Mobile phase B (acetonitrile) /% 0 0.00 400 99.0 1.0 1 3.00 400 70.0 30.0 2 6.00 400 60.0 40.0 3 9.00 400 60.0 40.0 4 15.00 400 40.0 60.0 5 19.00 400 1.0 99.0 6 23.00 400 1.0 99.0 7 23.01 400 99.0 1.0 C) Column temperature. 40 ° C;

D) Injection volume. 10 µL;

E) ionization source mode. electrospray ionization;

F) ionization source polarity. positive mode;

G) atomization gas. nitrogen;

H) atomization gas pressure. 0.28 MPa;

I) ion spray voltage. 4000V;

J) Dry gas temperature. 350 ° C;

K) Dry gas flow rate. 10 L/min;

L) Monitor the ion pair, the collision gas energy and the source fragmentation voltage, see Appendix B.

7.3.1.2 Determination of conditions for LC-MS-MS for pesticides and related chemicals in Group G

A) Column. ZORBAX SB-C18, 3.5 µm, 100 mm × 2.1 mm (inner diameter) or equivalent;

B) mobile phase and gradient elution conditions in Table 2;

Table 2 Mobile phase and gradient elution conditions

Total time/min Flow rate/(µL/min) Mobile phase A (5 mmol/L ammonium acetate water) /% Mobile phase B (acetonitrile) /% 0 0.00 400 99.0 1.0 1 3.00 400 70.0 30.0 2 6.00 400 60.0 40.0 3 9.00 400 60.0 40.0 4 15.00 400 40.0 60.0 5 19.00 400 1.0 99.0 6 23.00 400 1.0 99.0 7 23.01 400 99.0 1.0 C) Column temperature. 40 ° C;

D) Injection volume. 10 µL;

E) ionization source mode. electrospray ionization;

F) ionization source polarity. negative mode;

G) atomization gas. nitrogen;

H) atomization gas pressure. 0.28 MPa;

I) ion spray voltage. 4000 V;

J) Dry gas temperature. 350 ° C;

K) Dry gas flow rate. 10 L/min;

L) Monitor the ion pair, the collision gas energy and the source fragmentation voltage, see Appendix B.

7.3.2 Qualitative determination

When the sample is measured under the same experimental conditions, if the retention time of the detected chromatographic peaks is consistent with the standard sample, After the background of the sample mass spectrum, the selected ions are present, and the selected ion abundance ratio is proportional to the ion abundance ratio of the standard sample (Relative abundance > 50%, allow ± 20% deviation; relative abundance > 20% to 50%, allow ± 25% deviation; relative abundance > 10% to 20% Allowing ± 30% deviation; relative abundance <= 10%, allowing ± 50% deviation), you can determine the presence of this pesticide or related chemicals in the sample.

7.3.3 Quantitative determination

In this standard, liquid chromatography-tandem mass spectrometry was quantitatively determined by external standard-calibration curve method. To reduce the impact of matrix on quantitative determination, quantitative use the standard solution should be prepared using a standard solution of the matrix mixed standard solution. And to ensure that the measured samples of pesticides and related chemicals response value are within the linear range of the instrument. See Appendix C for the 448 Pesticide and Related Chemicals Multi-Reaction Monitoring (MRM) chromatograms.

7.4 Parallel test

Perform the parallel test of the same specimen according to the above procedure.

7.5 Blank test

Unless the sample is not weighed, according to the above steps.

8 Results are calculated and expressed

The results of liquid chromatography-tandem mass spectrometry were quantified by standard curve method. The quantitative results of standard curve method were calculated according to formula (1) Xi = ci × (1) M 1000 where.

Xi - Residue of test component in milligrams per kilogram (mg/kg);

Ci - the concentration of the solution to be measured from the standard curve, in micrograms per milliliter (µg/mL);

V - volume of sample solution in milliliters (mL);

M - The weight of the sample represented by the sample solution, in grams (g).

The result of the calculation should be deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are retained.

9 Precision

9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the Record the requirements of D.

9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with the Record the requirements of E.

10% limit and recovery rate

10.1 Quantitation limits

The quantitative limits of this method are given in Appendix A.

10.2 Recovery rate

When adding levels of LOQ, 4 × LOQ, add the recovery rate see Appendix F.

Appendix A

(Informative)

448 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration A.1 448 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration See Table A.1

Table A.1 448 kinds of pesticides and related chemicals, English name, method of quantitative limit, grouping, solvent selection and mixed standard solution concentration table

Serial number Chinese name English name quantitative limit/(µg/kg) solvent mixed standard solution concentration/(mg/L) Group A

1 Aniline Ling propham 110.00 Toluene 11.00 2 isoprocarb 2.30 methanol 0.23 3, 3, 4, 4, 3, 3, 3, 3, 3, 3, 5, trimethacarb 0.34 Methanol 0.03 4 ring amikron cycluron 0.20 methanol 0.02

5 Carbaryl 10.32 Methanol 1.03

6 Toxicant propachlor 0.28 Methanol 0.03 7 pimidazole raenzazole 1.34 methanol 0.13

8 West grass net simetryn 0.14 Methanol 0.01

9 Green Valley Long monolinuron 3.56 Methanol 0.36 10 times out of phosphorus mevinphos 1.56 toluene 0.16 11 azepine aziprotryne 1.38 methanol 0.14

12 Micronesia Secbumeton 0.08 Methanol 0.01

13 Azathione Sulfonamide cyprodinil 0.74 Methanol 0.07

14 Sulong Long buturon 8.96 Methanol 0.90 15 bisacyl chloride carbetamide 3.64 methanol 0.36 16 pirimicin pirimicarb 0.16 methanol 0.02

17 Isosubicin clomazone 0.42 Methanol 0.04 18 cyanocobalt cyanazine 0.16 methanol 0.02

19 Promised net prometryne 0.16 methanol 0.02

Potassium paraoxon methyl 0.76 Methanol 0.08 4,4-dichlorobenzhydryl 4,4-dichlorobenzophenone 13.60 Methanol 1.36 22 thiacloprid 0.38 methanol 0.04 23 imidacloprid 22.00 Methanol 2.20 24 sulfothiazide ethidimuron 1.50 methanol 0.15

25 Butoxalone isomethiozin 1.06 Methanol 0.11 26 oat enemy diallate 89.20 methanol 8.92

27 Acetochlor 47.40 Methanol 4.74 28 alkenone insects nitenpyram 17.12 methanol 1.71

29 Methoxypropine methoprotryne 0.24 Methanol 0.02

30 Dimethylphenol Meal dimethenamid 4.30 Methanol 0.43

31 Terracuria terrbucarb 2.10 Methanol 0.21 32 tebuconazole penconazole 2.00 methanol 0.20

33 Myclobutanil 1.00 Methanol 0.10 34 imazethapyr a imazethapyr 1.12 methanol 0.11 35 paclobutrazole 0.58 methanol 0.06 36 times thiophosphor sulfoxide fenthion sulfoxide 0.32 methanol 0.03 37 triazole alcohol triadimenol 10.56 methanol 1.06

38 Zhong Dingling butralin 1.90 methanol 0.19

39 Spiroxamine 0.06 Methanol 0.01

40 Methyl Formaldehyde tolclofos methyl 66.56 Methanol 6.66

41 Methanol 10.66 Methanol 1.07 42 allyl alcohol allethrin 60.40 methanol 6.04 43 diazinon 0.72 toluene 0.07

44 Paralyzed Phosphorus edifenphos 0.76 Methanol 0.08

45 Propoxamine pretilachlor 0.34 Methanol 0.03

Table A.1 (continued)

Serial number Chinese name English name quantitative limit/(µg/kg) solvent mixed standard solution concentration/(mg/L) Fluorosiliconazole flusilazole 0.58 Methanol 0.06

47 Propane Zinc iprovalicarb 2.32 Methanol 0.23 48 wheat rust Ling benodanil 3.48 methanol 0.35 49 fluoroamide flutolanil 1.14 methanol 0.11 50 sulfonamphan famphur 3.60 methanol 0.36

51 Benzoprene Benalyxyl 1.24 Methanol 0.12 52 benzyl chlorotriazole alcohol diclobutrazole 0.46 methanol 0.05

53 Acetiazole etaconazole 1.78 Methanol 0.18

54 Chlorophenylpyrimidinol fenarimol 0.60 Methanol 0.06

55 Tetramethrin 1.82 Methanol 0.18

56 Bacteriostatic dichlofluanid 2.60 Toluene 0.26 57 solution grass cloquintocet mexyl 1.88 methanol 0.19

58 Biphenyltriazole alcohol bitertanol 33.40 Methanol 3.34

59 Methyl chlorpyrifos methyl chloride

Potassium Diclofenac 10.99 Methanol 10.89

61 Ethyl oxalate clodinafop propargyl 2.44 Methanol 0.24

62 Suzumaru triflumuron 3.92 Methanol 0.39 63 isoxazolone isoxaflutole 3.90 methanol 0.39 64 paclitaxel anilofos 0.72 Methanol 0.07

65 Quixi Ling quizalofop-ethyl 0.68 Methanol 0.07

66 Fluorophenanthrene haloxyfop-methyl 2.64 Methanol 0.26

67 Benzylpyrone fluazifop butyl 0.26 Methanol 0.03

68 Ethyl bromothiophosphate bromophos-ethyl 567.70 Methanol 56.77

69 Scavenging bensulide 34.20 Methanol 3.42 70 bromophenylene phosphate bromfenvinfos 3.02 methanol 0.30 71 azoxystrobin 0.46 methanol 0.05

72 Pyridobacillus pyrazophos 1.62 Methanol 0.16

73 Fipronil flufenoxuron 3.16 Methanol 0.32

74 Indoxacarb 7.54 methanol 0.75

Group B

75 ethylene thiourea ethylene tiourea 52.20 methanol 5.22 76 butyric acid hydrate daminozide 2.60 methanol 0.26

77 Cotton Long dazomet 127.00 Methanol 12.70 78 nicotine 2.20 methanol 0.22 79 non-grass long fenuron 1.04 methanol 0.10 80 mice died crimidine 1.56 methanol 0.16 81 grasses molinate 2.10 methanol 0.21

82 Carbendazim 0.46 methanol 0.05

6-chloro-4-hydroxy-3-benzene Pyridazine 6-chloro-4-hydroxy-3-phenyl-pyridazin 1.66 methanol 0.17

84 Propoxur 24.40 Methanol 2.44 85 iszlone isouron 0.40 methanol 0.04

86 Chlorotoluron 0.62 Methanol 0.06 87 long-acting force thiofanox 157.00 methanol 15.70

88 Chlorobenzene chlorbufam 183.00 Methanol 18.30

89 Truffle Bendiocarb 3.18 Methanol 0.32

90 Fighting Chin propazine 0.32 Methanol 0.03 91 tert-butyl terbuthylazine 0.46 methanol 0.05 92 diuron 1.56 methanol 0.16

93 Chloromethylthiophosphate chlormephos 448.00 Methanol 44.80

94 Moisturizer a carboxin 0.56 Methanol 0.06

Butterothiophene 63.00 Methanol 6.30

96 Take the grass pronation 15.38 Methanol 1.54

Table A.1 (continued)

Serial number Chinese name English name quantitative limit/(µg/kg) solvent mixed standard solution concentration/(mg/L) 97 dimethamine dimethachloro 1.90 methanol 0.19

98 Bromoglyphine methobromuron 16.84 Toluene 1.68

99 Phorate 314.00 methanol 31.40

100 benzoate aclonifen 24.20 methanol 2.42 101 dean phosphorus mephosfolan 2.32 methanol 0.23

102 Benzylimidazole imibenzonazole-des-benzyl 6.22 Methanol 0.62 103 grass less long neburon 7.10 methanol 0.71

104 Knejiao Ling mefenoxam 1.54 Methanol 0.15 105 thiophosphate prothoate 2.46 methanol 0.25 106 ethofume sate 372.00 Methanol 37.20 107 different rice blast net iprobenfos 8.28 methanol 0.83

108 Tempe a TEPP 10.40 Methanol 1.04 Ciproconazole 0.74 Methanol 0.07 110 thiamethoxam 33.00 methanol 3.30 111 animal phosphorus crufomate 0.52 methanol 0.05 112 pyrimethazine etrimfos 37.52 methanol 1.88

113 Ketalyzes coumaretralyl 1.36 Methanol 0.14 Chlorpyrifos cythioate 80.00 Methanol 8.00 115 phosphamine phosphamidon 3.88 methanol 0.39 116 beetin phenmedipham 4.48 methanol 0.45

117 Bentonate Ester a bifenazate 22.80 Methanol 2.28

118 Cyclophosphamide fenhexamid 0.94 Methanol 0.09

119 Miconazole Flutriafol 8.58 Methanol 0.86 120 antibacterial propyl alcohol furalaxyl 0.78 methanol 0.08 121 bio-allyrin bioallethrin 198.00 methanol 19.80 122 benzonitrile phosphorus cyanofenphos 20.80 methanol 2.08

123 Methylpyrimidine Pirimiphos methyl 0.20 Methanol 0.02 124 buprofezin 0.88 methanol 0.09

125 Sulfonyl sulfone disulfoton sulfone 2.46 Methanol 0.25

126 Quinacid fenazaquin 0.32 Methanol 0.03 127 triazophos 0.68 Toluene 0.07

128 Frozen phosphorus DEF 1.62 Methanol 0.16 129 cyclic ester grass pyriftalid 0.62 methanol 0.06 130 metosterazole metconazole 1.32 methanol 0.13 131 mosquitoes ether pyriproxyfen 0.44 methanol 0.04 132 isoxacyl chloride isoxaben 0.18 methanol 0.02 133 furazanil flurtamone 0.44 methanol 0.04 134 trifluralin 334.80 toluene 33.48 135 methyl wheat straw fluoride isopropyl ester flamprop methyl 20.20 methanol 2.02

136 Bio-Benzfurantee bioresmethrin 7.42 Methanol 0.74 Propiconazole 1.76 Methanol 0.18 138 chlorpyrifos 53.80 methanol 5.38

139 Ethyl Chlorofluoxane fluchloralin 488.00 Methanol 48.80

140 Chlorsulfuron a chlors...

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Referenced standards

Cited by

GB 2763-2026National food safety standard-Maximum residue limits for pesticides in food

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